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Ceramics International 42 (2016) 1573915746

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Ceramic protection plates brazed to aluminum brake discs


L. Gorjan a,n, M. Boretius b, G. Blugan a, F. Gili c, D. Mangherini c, X. Lizarralde d, M. Ferraris e,
T. Graule a, A. Igartua f, G. Mendoza f, J. Kuebler a
a
Empa Swiss Federal Laboratories for Materials Science and Technology, Laboratory for High Performance Ceramics, berlandstrasse 129, 8600 Dbendorf,
Switzerland
b
Listemann Technology AG, Wirtschaftspark 34, P.O. Box 247, LI-9492 Eschen, Liechtenstein
c
CRF Centro Ricerche Fiat, Strada Torino 50, Orbassano, Italy
d
Fagor Ederlan Edertek, Garaia Berrikuntza Gunea, Isasi Kalea, 6 Posta K. 19, 20500 Arrasate-Mondragn, Gipuzkoa, Spain
e
POLITO Politecnico di Torino, DISAT Department of Applied Science and Technology, Corso Duca degli Abruzzi 24, I-10129 Torino, Italy
f
IK4 TEKNIKER, Parke Teknologikoa, Calle Iaki Goenaga 5, 20600 Eibar, Gipuzkoa, Spain

art ic l e i nf o a b s t r a c t

Article history: Aluminum alloys are light-weight and one of the most interesting material solutions to optimize the
Received 3 May 2016 strength/weight ratio to reduce car weight; however they are also relatively soft and therefore cannot be
Received in revised form used for intensive wear applications. We developed an aluminum alloy part combined with hard and
5 July 2016
wear-resistant Al2O3-based ceramic plates on the surface for demanding mechanical parts for automotive
Accepted 5 July 2016
industry such as disc brakes.
Available online 7 July 2016
Tribological tests of various engineering ceramic materials were performed in order to nd a ceramic
Keywords: material with a combination of coefcient, wear resistance and thermal energy dissipation for the car
Ceramic brakes. Al2O3-based ceramic showed promising properties, as well as being cost effective.
Wear resistant
Two different approaches to braze ceramic on aluminum were investigated. A two-step brazing
Soldering
process using Cu-Sn-Ti-Zr ller alloy and a single step ultrasonic active soldering with Sn-Ag-Ti ller
Brazing
Aluminum brake disc alloy. Larger areas of aluminum could be covered with a segmented brake design in which many ceramic
plates were joined surface. Comparable tribological properties to those of the bulk ceramic material were
achieved.
& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

1. Introduction Brazing and soldering are preferred joining techniques when a


strong, thermal conductive, temperature and solvent resistant
There is a strong interest in the automotive industry to obtain joint is required. This approach has an additional advantage re-
lighter components in order to improve energy efciency and garding the surface protection of soft aluminum, because it en-
emission output. The amount of aluminum, used in passenger cars ables to attach a material which was made in a separate process
has risen signicantly in the past decades, which resulted in im- to have well-dened and optimized properties for the desired
proved energy efciency. It is used in many different components application.
like wheels, engines, heat exchangers, transmission and others. In the past other ways to improve the aluminum surface have
This is possible, because aluminum alloys have several good been explored. Typically the surface is improved by applying hard
properties like high strength to weight ratio, excellent thermal and wear resistant coating on the surface. For example ferrous
conductivity, corrosion resistance and they are easy to machine thermal spray coating [1]. Especially with micro-arc oxidation a
and recycle. However, they are relatively soft and offer insufcient very hard and strong layer of Al2O3 coating can be prepared [25].
wear resistance for applications where intensive friction is pre- Although very good properties were achieved, these promising
sent. In this paper, an idea to combine a tough and light-weight technologies are not the focus of this paper.
aluminum body with a hard and wear-resistant ceramic, layer Brazing and soldering of ceramic to aluminum alloys is not a
joined at the surface, is explored and evaluated for applicability to well-established and proven technology. There are two major
automotive disc brakes. reasons for that. First, brazing ceramic to aluminum is difcult
because molten ller metal does not spontaneously form a strong
n
Corresponding author. bonding to the surfaces, especially at the relatively low tempera-
E-mail addresses: lovro.gorjan@empa.ch, lovro.gorjan@gmail.com (L. Gorjan). tures which are required to join aluminum alloys. Filler alloys with

http://dx.doi.org/10.1016/j.ceramint.2016.07.035
0272-8842/& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
15740 L. Gorjan et al. / Ceramics International 42 (2016) 1573915746

a so called active element (most commonly Ti or Zr) are used to


braze ceramics. Only moderate bonding strengths (15  30 MPa)
were reported by using hot pressing of Al2O3 to aluminum at
600 C in vacuum using alloys without an active element such as
Al-Si and Al-Cu [6]. When ller alloy contains an active element it
can react with the ceramic surface and forms strong chemical
bonding [717]. The modied surface then enables the wetting of
the molten ller. The addition of rare earth elements, such as Ce
and Ga also improves wettability, while it also improves strength
[18] and the oxidation resistance of the metal in molten state
[19,20]. Relatively high temperature is typically needed for the
activation of the active element. For example a temperature in
excess of 700 C is needed to achieve good wetting of the Sn-Ag-Ti
alloys on Al2O3 ceramic [13,14,20,21]. However, high temperature
presents a problem for joining aluminum alloys since cast alumi-
num alloys have relatively low melting points (o600 C) and their
properties can be compromised at higher temperatures.
The second major challenge in brazing or soldering ceramic to
aluminum originates from the different shrinkages of both mate-
rials after the cooling to ambient temperature. Large thermal Fig. 1. Sketch of an aluminum braze disc protected by wear-resistant hard material.
stresses are generated which can compromise the mechanical
properties of the composite product. In order to avoid this in- Table 1
herent problem a sophisticated graded material structure or spe- List of selected materials used in the research.
cial design in size and shape could potentially avoid the critical
Material Composition Density [g/ CTE Thermal con-
issues.
cm3] [10  6/K] ductivity [W/mK]
For applications like brake discs, a high precision surface at-
ness and parallelism is required, which can most likely be only A380 Al 8.5Si 3.5Cu 2.71 22 96
achieved by nal grinding, after the ceramic parts have already A356 Al 8.5Si 0.3Mg 2.69 22 160
been soldered on the aluminum frame. During such a mechanical Al2O3 99.7% Al2O3 3.93 7.0 27
Al2O3-SiC 99.99% pure 3.84 6.8 24
operation possible defects are introduced on the surface of stres- Al2O3 5 vol% SiC
sed ceramic. An additional important aspect of the research was TZ3Y ZrO2 5% Y2O3 6.1 10 2
also the price of the nal composite. Only cost effective products Mullite 3Al2O3 2SiO2 3.1 5 6
would be acceptable for automotive mass application. SiC SiC 3.2 4 120
ZTA Al2O3 8 vol% TZ3Y 4.2 8 20
In this work the development of composite materials for disc
brakes and possibly other friction intensive applications are pre-
sented. First a material with the desired friction characteristics Table 2
was selected for the outer layer of the composite. Then different List of materials used for joining.
joining techniques were considered to prepare aluminum/ceramic
composite. Material Type Composition [wt%] Melting temperature [C]

GS220 Solder alloy 92Sn 3Ag 3Ti (Ce, Ga) 220  230
Diabraze Braze alloy 74Cu 14.5Sn 10Ti 1.5Zr 868  925
2. Experimental

2.1. Concept design alloy with the composition of 92Sn3Ag3Ti ( Ce, Ga). It has a
melting range of 220230 C and it contains titanium as an active
The idea behind the project was to use an aluminum alloy to element.
make a lightweight brake disc body and cover the wear area with a Diabraze is Cu-Sn-based active ller metal and was chosen
hard and wear-resistant material. The concept is schematically because of its high strength and ability to wet and react with
shown in Fig. 1. Cast aluminum alloy is used for a body onto which materials which are typically difcult to bond by brazing [2224].
harder and wear resistant ceramic material is brazed. The good bonding is due to the large amount of the active ele-
ments Ti and Zr. Diabraze has been already successfully used to
2.2. Materials join diamond and boron nitride ceramics with steel substrate
[22,24].
Materials used in our research are listed in Table 1 together
with their basic properties. Two different aluminum alloys were 2.3. Joining and machining the samples
used - A380 and A356, which are widely used in automotive and
other industries. Solid sample parts were cast at Fagor Ederlan, Two different approaches to bond wear resistant material on
Spain, using a low-pressure aluminum casting process. top of aluminum part were considered and are sketched in Fig. 2.
Several technical ceramic materials were considered for the top a) Two-step vacuum brazing was made using the Diabraze
layer. After the tribological tests of different bulk ceramic samples CuSnTiZr braze metal (Fig. 2a). First, the alloy slurry was applied to
we focused on Al2O3 ceramic. Material marked as Al2O3 was pre- the ceramic surface and processed at 900 C in vacuum in order to
pared from commercial 99.7% alumina powder (Granalox NM9922, melt the ller metal and make a strong bonding with the ceramic
Nabaltec, Germany), pressed and sintered at 1620 C for 2 h in air. surface. After the end of this metallization step, the samples were
Materials used for joining wear resistant layers to aluminum put on the top of aluminum alloy substrate so that the metalli-
alloy substrates are listed in Table 2. zation layer was in direct contact with the aluminum alloy. The
GS220 (MBR Electronics, Switzerland) is an active soldering samples were then heated in vacuum to 555 C for 15 min. This
L. Gorjan et al. / Ceramics International 42 (2016) 1573915746 15741

Fig. 2. Different approaches to apply hard material on the surface of aluminum alloy part by brazing or soldering.

temperature is actually far below the solidus temperature of the resistance of the joint is lower, due to the relatively low melting
braze alloy (868 C) because we are limited by the melting point of point of the solder alloy. To further reduce the thermal stresses we
the aluminum alloy substrate, which has a melting range of 555 also explored the so called segmented design, where large surface
615 C. However holding at the solidus temperature of the sub- of aluminum is covered by multiple smaller pieces of ceramic.
strate, the braze alloy reacts with the aluminum, forming a bond. After joining the surfaces were ground by diamond wheel in
The joining procedure was developed and made by Listemann order to achieve the proper atness required for the tribological
Technology AG, Liechtenstein. tests. Final surface roughness Ra was 1.1 mm as measured by a
The braze alloy has a relatively high melting point and thus Hommel tester T500 (Hommelwerke, Germany).
guarantees temperature resistance of the joint. On the other hand
the process involves relatively high processing temperatures 2.4. Characterization
which causes large thermal stresses upon cooling to room
temperature. Apparent shear strength was determined by a single-lap ap-
b) Direct soldering was performed using the SnAgTi(Ce, Ga) parent shear test sketched in Fig. 3a. Samples were prepared from
solder alloy. Soldering was made with the ultrasonic soldering 6  6  2 Al2O3 ceramic plates joined on 12  12  13 mm alumi-
system (USS-9510, MBR Electronics, Switzerland) using a 6 mm num blocks. The test was performed with a Zwick Z005 (Zwick,
diameter tip. Such joining was successfuly used in our recent re- Germany), universal testing machine with a constant deformation
search on joining ceramic to aluminum alloy [17]. Cleaned samples rate of 0.5 mm/min and with the recording of the applied force.
(10 min in acetone lled ultrasound bath) were heated to 260 C Apparent shear strength was simply calculated as a maximum
and solder alloy was melted on both surfaces, ceramic and alu- force divided by the joint surface area.
minum. The wetting of the solder was promoted with the sol- Tribological characterization was carried out with the pin on
dering tip with 15 W of ultrasound power at 40 kHz. The tem- disc laboratory scale testing apparatus at Centro Ricerche Fiat
perature of the tip was 260 C and the time of ultrasonic assisted (CRF), Italy as shown in Fig. 3b. The applied force was 200 N and
wetting was 15 s. Both parts were then joined together, positioned the rotational speed of sample was 850 rpm. Total time of the test
and cooled down in air to ambient temperature. Since the sol- lasted 900 s. Air cooling system was used to simulate car brakes
dering is done at a relatively low temperature the thermal stresses during running vehicle. The temperature on the sample surface
are smaller than in the case of brazing. However, the thermal was measured with a pyrometer. Two different counterpart pad

Fig. 3. Sketch of an apparent shear test (a) and tribological test (b).
15742 L. Gorjan et al. / Ceramics International 42 (2016) 1573915746

materials were used for the tests; a) a reference pad material ty-
pical for cast iron disc brakes supplied by CRF and b) a harder type
of pad material supplied by Edertek.

3. Results and discussion

3.1. Bulk materials characterization

Tribological tests of bulk materials were used as a rst test to


select the most appropriate candidate materials for the top layer.
Cast iron was also tested as a reference; in combination with soft
pads it is used in the industrial production of car brakes. According
to the industrial experience in CRF the optimal coefcient of fric-
tion should be between 0.35 and 0.55. The surface temperature
during breaking should be as low as possible. The tribological re- Fig. 5. Microstructure of sintered, polished and thermally etched Al2O3 ceramic.
sults of bulk ceramic materials are shown in Fig. 4. The region of
acceptable conditions is marked in Fig. 4. Tribological tests showed
that the soft pads exhibit too low coefcient of friction. Relatively diffusion layer was 2 mm thick. We could not nd any con-
high temperature was measured at the surface of mullite and centrated areas of Sn.
zirconia. This is due to the low thermal conductivity of the two Smaller ceramic samples (6 mm  6 mm  2 mm) could be
materials. The heat generated during friction cannot quickly dis- joined without cracks. Samples were tested for apparent shear
sipate through the ceramic layer. Hard pads in combination with strength evaluation and in all cases the ceramic part did not crack
Al2O3, Al2O3-SiC and ZTA showed good properties. during the test. The typical fracture surfaces after the test are
According to the tribological results made with bulk materials, shown in Fig. 7. The joint failed quite far away from the ceramic
our further research focused on Al2O3 because of the best overall surface, in the Cu-diffusion zone as can be seen from the side view
properties and also relative low price. In combination with hard of ceramic part after the test. Thick chunks of residual metal were
pads it showed the most promising tribological behavior for the still attached on the surface.
brake application. The microstructure of Al2O3 ceramic is shown in Cohesive failure inside the reaction zone was identied as a
Fig. 5. mechanism of failure. Average apparent shear strength was
42 MPa with a standard deviation of 8 MPa (see Fig. 10). This is
3.2. Two-step direct vacuum bonding of ceramic to aluminum considerably lower than the reported values in the literature for
the yield strength of such an alloy which should be 550 MPa [22].
Metallization of the ceramic surface and subsequent joining at The failure of the joint actually goes through the Cu-diffusion zone
550 C in vacuum resulted in apparently good joints. However, with unknown properties that also contains large cavities. Cavities
after metallographic analysis it was revealed, that all ceramic parts can act as a strength determining aws. Moreover, large residual
with 20  10 mm  2 mm in size were cracked. A typical micro- thermal stresses after cooling to ambient temperature, can con-
graph of a joint is shown in Fig. 6. A distinct layer ( E50 mm thick) siderably reduce the strength of the alloy by introducing micro-
near the ceramic surface was made of mixed Al and Si2Ti phases. cracks [25]. All the mentioned factors can explain the low strength,
ZrO2 grains were found at the ceramic surface. The titanium was although the precise contribution of each factor is difcult to
spread all over the thin layer, but it did not diffuse into the alu- quantify.
However, the results also show that the wetting and the ad-
minum substrate. However, the layer was almost depleted of
hesion of ller metal to the ceramic is relatively strong. Optimizing
copper which diffused deeply into the substrate, forming a CuAl
the process would possibly lead to a diffusion zone with smaller
phase between the aluminum grains. In some areas the Cu
voids and higher shear strength of the diffusion zone. But the
cracking of large ceramic parts is not expected to be solved just by
optimizing the processing conditions. In order to join larger parts
without cracking a ller alloy with a lower melting point is re-
quired. That is the reason to investigate the joining with Sn-Ag-Ti
active solder with a melting range of 220230 C. It is also well
known that the amplitude of residual stresses signicantly depend
on the dimension of the parts [25,26]. Joining parts with larger
interface areas result in larger residual stresses. Therefore, by
choosing a smaller ceramic piece, the cracking due to thermal
stresses can be potentially avoided.

3.3. Directly joined ceramic to aluminum by ultrasonic soldering

Al2O3 ceramic was successfully joined to the aluminum alloy


substrate by ultrasonic soldering with Sn-Ag-Ti active ller alloy. A
typical microstructure of the cross section is shown in Fig. 8. The
thickness of solder layer varied from 30 to 50 mm for different
samples and no pores or other larger defects were found in the
Fig. 4. Coefcient of friction and surface temperature during tribological tests for
different ceramic materials and iron as a reference. Red rectangular show the re-
joint layer. A very sharp and well dened interface between the
gion in which both the coefcient of friction and the temperature are good for the ller metal and aluminum substrate with no diffusion region was
car brake discs. observed. Silver-rich components were mostly concentrates at the
L. Gorjan et al. / Ceramics International 42 (2016) 1573915746 15743

Fig. 6. Low magnication cross section micrograph of Al2O3 joint to aluminum alloy in a two-step vacuum process using CuSnTiZr braze alloy is shown in g. a). Elements
were identied by EDX analysis. Figure b) shows a magnied interface area between ceramic and ller metal.

Fig. 7. A shear fracture surfaces on the aluminum side (a) and on the ceramic side (b). A rough metallic surface left over was found on both sides. The residual metal is also
clearly seen from the side view of ceramic part (c).

solder/aluminum interface. Tin/titanium intermetallic grains were detachment of ller alloy from the ceramic surface. Typical shear
found through the braze layer. fracture surfaces are shown in Fig. 9. Large areas of exposed
Single-lap apparent shear strength was measured on samples ceramic were found; a consequence of the adhesion failure during
with 6  6  2 mm3 Al2O3 plates soldered on a 12  12  13 mm3 the shear test. In other areas residual solder alloy was found on the
aluminum alloy block. Two mechanisms of fracture were ob- ceramic surface. It was conrmed by EDX analysis that the residual
served: a) the cohesive failure of the ller alloy and b) the metal is solder alloy and not aluminum alloy which is in
15744 L. Gorjan et al. / Ceramics International 42 (2016) 1573915746

showing higher coefcient of friction and a relatively long initial


phase in which coefcient of friction is not stable (Fig. 12). After
analysis of the friction surface of the sample, it was determined
that some edges were slightly sticking out of the at plane. Also
some solder material was spread from the junctions between the
ceramic plates (Fig. 11d). The topological irregularity must have
occurred after the grinding, due to a stress-releasing deformation
in the aluminum alloy substrate. This caused an additional friction
resulting in an increased measured coefcient of friction. During
the tribological test the temperature at the surface reached 140 C,
which is relatively high for a solder with a low-temperature
melting point. Therefore, thermal stresses might have caused de-
formation and slight repositioning of the ceramic plates and con-
sequently the increase in the coefcient of friction.
Another sample (marked as the sample 2) with smoother
transitions between the segments, showed similar friction prop-
Fig. 8. Micrograph of polished cross section of soldered Al2O3 to Aluminum alloy
sample with. Elements identied by the EDX analysis are shown.
erties as those of the monolithic single piece of Al2O3 ceramic. This
demonstrates that similar friction behavior as in the case of bulk
agreement with cohesive failure of the solder mechanism. Average material can be made with the segmented design if the nish of
apparent shear strength was 50 MPa with a standard deviation of the surface is properly done. The surface quality can be a critical
12 MPa (Fig. 10). The large scattering was connected to the scat- issue for the plated design in applications where coefcient of
tering of the percentage of cohesive failure area the larger the friction must be precisely dened. No wear of ceramic or change in
area, the higher the strength. surface roughness could be detected; similar surface as produced
For tribological testing larger parts were required. Attempts to by the diamond grinding process remained after the test.
make a tribological sample with 54 mm diameter single ceramic
disc plate, soldered onto 5 mm thick aluminum alloy disc substrate 3.4. Demonstrational brake disc
failed due to the cracking of the ceramic after cooling to ambient
temperature. Even though the temperature difference between the In order to demonstrate the possibility of scaling-up and cov-
solidus of the solder and the ambient temperature is only around ering even larger areas of aluminum surface, a half-scale alumi-
200 C, thermal stresses are large enough to cause cracks in num brake disc covered with Al2O3 ceramic plates was made by
ceramic (Fig. 11b). ultrasonic soldering with Sn-Ag-Ti active alloy. The photograph of
A solution was found in the segmented design where the sur- the part is shown in Fig. 13.
face is covered with many ceramic plates. In this way we could
obtain a crack-free 54 mm diameter discs for tribological tests
(Fig. 11b). For additional reliability a design with side support rim 4. Conclusion
was chosen. The ceramic plated surface was ground with a dia-
mond blade before the tribological testing to achieve proper at- Different technical ceramic materials were investigated as a
ness and parallelism for the tribological testing. Surface roughness wear protection layer for aluminum alloy car brake discs and
parameter Ra after the grinding was 1.1 mm. possibly other friction intensive wear application. Al2O3 proved to
Tribological properties of the bulk Al2O3 was compared with have good tribological and thermal properties for the application;
the segmented sample under continuous pin on disc mode, however the joining of Al2O3 to aluminum substrate presents

Fig. 9. Fracture surfaces on the aluminum side (a) and on the ceramic side (b). Mixed failure mechanism was observed. Cohesive failure of solder layer and detachment of
solder from ceramic surface.
L. Gorjan et al. / Ceramics International 42 (2016) 1573915746 15745

Fig. 10. Apparent shear strengths of 6 mm  6 mm Al2O3 samples soldered by Sn-Ag-Ti solder alloy or brazed by Cu-Sn-Ti-Zr alloy are presented in a). Bars present average
value and vertical line present standard deviation. Typical stress-strain curves are shown in b). Black lines are for Sn-Ag-Ti soldered samples and grey-dashed lines are for
Cu-Sn-Ti-Zr brazed samples.

major challenges. Two different approaches for joining were ca. 6  6 mm2) part to aluminum, the ceramic is cracked during
investigated. the joining process.
Although the two steps vacuum brazing with Diabraze Cu-Sn- Using the lower melting point Sn-Ag-Ti active solder a crack
Ti-Zr braze forms a good bonding to the ceramic surface, the free bonding can be achieved for ceramic plates with size of
thermal stresses are so large that when brazing a large ceramic (4 20 mm  20 mm. Larger areas can be covered by multiple plates;

Fig. 11. Photograph of cracked disc after soldering made from one ceramic piece (a) and crack-free disc with segmented ceramic cover soldered on aluminum alloy substrate
(b). The disc after the tribological test is show on photo c) with clearly visible tribo-layer deposited from the friction with the pad. The detail of tribolayer at the edge between
two ceramic plates is shown in gure g).
15746 L. Gorjan et al. / Ceramics International 42 (2016) 1573915746

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(FP6, MA-TERA/HPE-2227), nanced by the Swiss Commission of 130136.
Technology and Innovation (CTI) under contract no. 12128.1 PFIW- [25] K. Suganuma, Joining ceramic and metal, in: S. Somiya (Ed.), Handbook of
Advanced Ceramics, Elsevier, Amsterdam, 2013,
IW and MIUR (Ministero dellIstruzione, dellUniversit e della pp. 775788, http://dx.doi.org/10.1016/B978-0-12-385469-8.01001-7.
Ricerca) Italy under the contract Decreto n. 698/ric17/10/2012, by [26] K. Sagunama, T. Okamoto T, M. Koizumi, Inuence of shape and size on re-
the CDTI Spanish (Contract IDI-20120133) and SPRI Basque re- sidual stress in ceramic/metal joining, J. Mater. Sci. 22 (1987) 35613565.
gional research Agencies.
Website of the Jolie project: http://www.composites.polito.it/?
p projects_european_jolie.